Process of hydrogenating oil mixtures and the like.



0. ELLIS; PROCESS OF HYDROGENATINGOIL MIXTURES AND THE LIKE APPLICATIONIILED SEPT. 10, 1912.

tented Nov Inventor Attest Q. g

' tank 1 is given a rotary motion While the- CARLETON ELLIS, 0FMONTCLAIR, NEW JERSEY.

PROCESS OF HYDROGENATING OIL MIXTURES AND THE LIKE.

Specification of Letters Patent.

Application filed September 10, 1912.. Serial No. 719,541.

To all whom it may concern:

Be it known that I, CARLETON ELLIS, a citizen of the United States, anda resident of Montclair, in the county of Essex and State of New Jersey,have invented certain new and useful Improvements in Processes ofHydrogenating Oil Mixtures and the like, of which the following is aspecification.

This invention relates to an oily or fatty product preferably 0rspecifically consisting of a mixture of treated oils or fats and to theprocess of making same all as more fully hereinafter described and asclaimed.

Reference to the accompanying diagrammatic drawings makes clear themanner in which the process herein may be carried out.

In the drawings Figure 1, shows a treating tank in vertical section,while Fig. 2 illustrates by sectional view a modified form of apparatusapplicable in the treatment of certain fats.

Like reference characters designate like parts throughout.

In Fig. 1, a treating tank 1 (preferably cylindrical) is surmounted by aspraying dome 2. The tank is provided with the heating jacket 3, oilinlet pipe 4, gas exhaust pipe 5, plugged aperture 6, oil outlet pipe7,.and manhole 8. The dome 2 also is provided with a manhole 9. 10 is agas exit, at which point the intake of the pump 11 communicates with theupper part of the tank 1. From this pump a delivery pipe 12 extends tothe bottom-of the tank and connects with the gas distributers 13 and 14which are tubular in form and are situated in preferably radial positionat or near the bottom of the tank. Outlets or nozzles preferablylaterally disposed-afford exits for the gas into the tank at this point.A larger number of outlets or nozzles is provided on one side of eachdistributer than on the other. Thus by the greater lateral ejection ofthe gas on one side than on the other the body of oil largely fillingthe lesser number of opposing jets on the opposite side of thedistributer being directed into and against a constantly advancingcurrent of oil afiord a degree of impingement which greatly lends to thehydrogenafatty mixtureto be entered thereinto. 1s a pump whose inletcommunicates with tion of fatty mixtures diflicult of rapid treatment inother ways. This opposed differential ejection of the gas thereforeconstitutes an important feature of the apparatus involved in theprocess as concerned under Fig. 1. 15 is a branch outlet gas pipeleading from the pump 11 to the inspirators and atomizers 16, andterminating as concentrically disposed nozzles 21 with in the saidinspirators. A pipe 17 extends from near the bottom of the tank to theseinspirators and enables the oil or 18 the pipe 17 and whose outlet bymeans of the pipe 19 connects with the inspirators 16. In the lower partof the dome are a series of screens or perforated metal sheets 20 spacedslightly apart. At 20 are shown plpes for Patented Nov. 11, 1913.

the admission of superheated steam for decolorizing purposes orotherwise as will be hereinafter set forth.

In the operation of the process in accordance with Fig. 1 the oilymaterial is entered by the pipe tuntil the tank is about two-thirdsfilled. Steam ispassed through the jackets 3 to heat the oil to thetreating temperature. Any air contained in the tank and connections ispreferably removed by passing hydrogen or water-gas therethrough whilethe oil is being treated. Catalyzer, preferably in a very finely dividedform is entered by the aperture 6. The operation of the pump 11 causesgas to be withdrawn from the top of the tank and to be propelled intothe distributers 13 and 14 and from thence. into the body of oilymaterial causing rotation thereof and differential impingement asaforesaid. Gas passing through the pipe '15 into the in spirators 16causes oily material and catalyzer to be propelled from the bottom ofthe tankfl into the inspirators. The material mingles with the gas andis ejected from the inspirators. These as shown are arranged radiallyopposed so that the atomized jets mutually impinge and the componentparts of the jets thus become furthercommingled. The oil fog produced,in its atmosphere of hydrogen passes through the screens 20 and throughthe special heating zone engendered by the heating pipes or coil 20,finally collecting in the tank 1. This cycle is repeated or continueduntil the material hasbecome hydrogenated to thedegree desired, when thetank is emptied'of its oily contents by the outlet 7. Optionally thepump 18 may be used to cause .a more rapid circulation of the oilymaterial, but when the catalyzer -is of a gritty nature, 'abrasiveaction may preclude such use. Gritty particles do not,

33 however, interfere with the operation of the'- inspirators 16 underthe gas pressure developed by the pump 11.

' As indicated, the apparatus of Fig. 2 is perhaps of more specificapplication'than that of Fig. 1 in carrying out the process ofthe'present invention. -In Fig. 2, l is a treating tank preferably asshown of conical shape. It is provided with a stationary mass ofcatalyzer'3l resting on a grid 29. 32 is a manifold carrying a series ofdownwardly depending nozzles or atomizers. is an upwardly directed et ornozzle for entry of hydrogen gas. In theoperation .of theprocesshereunder oil is continuously .circulated 5 by means of the pump18 through the porous l bed of catalyzer 31. The spraying device 32enables theoil in a finely divided conditionto come into intimatecontact with the catalyzer and the counter-current of hydrogen 3 orsimilar gas. A heating zone preferably somewhat localized is maintainedby the heating pipes 20 The coning or taper of 'the tank is preferablyadjusted so thatthe mass of catalyzer contracts with respect to 35 thedegree of gradual agglomeration of the spray particles, thereby enablingthorough contact of the oily material, gas and catalyzer to effectivelytake place.

While the foregoing process is applicable .40 to the-treatment of 'oilsof a unitary chemical composition it is more particularly orspecifically adapted to the hydrogenation of.

hydrogen addition throughout the ,several.

- unsaturated bodies which may have been present in the raw mixturesapparently cannot be carried out by the present'known methods ofhydrogenation in a thoroughly I controllable manner as is possible witha unitary body such as oleic ac d. The present process enables suchmixtures of oily material to be readily hydrogenated to the desiredextent, and in a certain measure en- '66 ables selective hydrogenationto be under tration it may be stated that palm oil which is practicallyunfit for edible purposes owing to'its rank odor 'anddisagreeable tastemay be, converted into a clean smelling fat possessing a faint spicy tocoffee-like odor and improved flavor. -So persistent is the odor ofordinary palm oil that when made into soap the saponified productretains the original disagreeable odor of the oil unchanged. By myprocess palm oil may be so freed from odor that it cannot be recognized'in soaps by odor and the hydrogenated and saponified product yields animproved lather and detergent properties of a desirable character. Thepotash and soda soaps are especially .useful. A suitable soap may bemade by hydrogenating a mixture of equal parts cotton-seed and palm oiland 5 saponifying 1Q0 parts of this mixture with 11 parts of causticsoda and 13 parts of caustiepotash. Other soap stock mixtures are palmoil 1 part, cotton-seed oil 3 parts; palm oil 1 part, corn-oil 2 parts,tallow l part; palm oil 1 part, horse fat 1 part and cotton-oil foots ordistilled fatty acids 1 part. Owing to the albuminous matters and largeproportion. of free acids and other bodies produced by rancidification,palm oil 5 is destructive to some catalyzers. Palm oil oftentimes showsafatty acid test indicative of a "50% or more of free fatty acids. It isnot desirable to hydrogenate with this high proportion of acids presentfor the best re- 1 sults, but preferably theacidit of the oil should-notexceed 25 or 30%. y diluting a high acid oil with an 'oil with which it1s to be asss'ociated ultimately in edible products, soaps 0rother-materials, action on the catalyzer is reduced to a minimum. In thecase of nickel catalyzer or other similar metal catalyzer present inafinely divided condition an oil having this excess of free fattyacid isobjectionable, because of the possibility of solution of the nickel orother metal by the acid, especially when hydrogenatin at a hightemperature and in such'a case the free acid should be reducedproportionately. For hydro-genating at relatively low tempera tures, thepresence of 20 to 30% of the free fatty acid does no harm'according tomy experimental observations. I have found rancid palm oil running up to30 to 33% of free fatty acid to hydrogenate very rapidly even at atemperature of 190 in the apparatus described in my U. S. Letters PatentNo. 1,026,156 of May 14, 1912. Palm oil is capable of being decolorizedby heating, a temperature of 240 or higher being used for this purpose.Decolorization atthis high temperature especially in the presence of airor oxygen leads to further decomposition of the oil and increasedformation of free fatty acids. By decolorizing in an atmosphere of aninert gas further rancidification is substantially prevented. Hydrogenis suitable for this purpose so that the operation of decolorization andhydrogenation may be carried out simultaneously to advantage. I

For the manufacture of edible oils it is undesirable to continuouslyheat the oil to the decolorization temperature which in the case of palmoil in the presence of hydrogen is about 190 C. By the present process adeeoloring zone of somewhat higher temperature may be maintained locallyin the apparatus and while the major portion of the hydrogenationnormally goes on at the desired relatively low temperature, the lo-'calized heating zone effects the decolorization under perfectlycontrollable conditions. Sometimes the treating tank has, however, to bereduced in temperature after hydrogenation and decolorization have goneoh to some extent, and for this purpose a cooling fluid may be passedthrough the heating jacket shown in the Fig. 1, while maintain y, ingthe high temperature heating zone within the mass of screen material inthe atomizing dome. At a temperature of 190 maximum, palm oil of about25% or so acidity is hydrogenated to bring its original titer 86.4 F. upto 968 F. and the color is changed from a deep orange to a pale yellow.An intermediate body having a titer of 91 is suitable for and as anaddition to other oils in the manufacture of butter substitutes. Thetiter herein is that of the oil and not that of the fatty acid. Theproduct of a titer of 96.8" F. makes an excellent soap material and thesoap produced is free from the disagreeable odor of crude palm oil.

Wheret er the term oil or fat has been used herein, it should beunderstood that for the purpose set forth these terms are used assubstantially synonymous.

The gas pressure which may be employed in treating the oil or fat inaccordance with the present process is variable depending upon thecharacter of the product required. In the manufacture of edible productslow pressure and low temperatures preferably should be employed in orderto avoid the formation of lactones. However, these depend to a-certainextent on the oil-which is being treated and the temperature andpressure may therefore be regulated with respect to this consideration.In the manu- Chinese wood, caster, cocoanut, sesame, soy

bean, and other vegetable oils separately or in. admixture may beeflectively treated;

also marine oils such as menhaden, codl-iver oil, whale oil and otherfish oils; also animal oils such as oleo-stearin, tallow and lard oil,horse oil, tankage greaseoil foots and the like. Oil foots are usuallyvery difiicult to hydrogenate owing to the high percentage ofimpurities, some of which act as a poison on catalyzers under mostcircumstances. By dilution of foots with 2 or 3 parts of oil witlrwhichthe foots are ultimately to be associated, as in soap, lubricants andthe like, the hydrogenation process often may be carried out with ease.Thusioils and fats which are so impure as to ,be practically incapableof hydrogenation land which are furthermore often incapable of beingrefined without excessive cost, may, under'the present process, behydrogenated without any especial preliminary refining, it being onlynecessary to determine the ultimate use of the impure oil and the extentto which it is to be incorporated with other oils and to then make acomposition approximating this composition and hydrogenate same.

' What I claim is 1. The process of hydrogenating composite fattymaterial and the like which comprises diluting an acid oil with asubstantially neutral oil and in subjecting the mlX- ture to hydrogen inthe presence of a catalyzer.

2. The process of hydrogenating composite fatty material and the likewhich comprises diluting an acid oil with a substantially neutral oiland in subjecting the mixture to a hydrogen-containing gas in thepresence of a catalyzer.

3. The process of hydrogenating composite fatty material and the likewhich comprises diluting a substantially catalyzertoxic oil with asubstantially neutral oil and in subjecting the mixture to ahydrogencontaining gas in the presence of a catalyzer.

4. The process of hydrogenating composite fatty material and the likewhich comprises diluting a substantially catalyzertoxic oil with asubstantially neutral oil and in subjecting the mixture to ahydrogencontaining gas under pressure in the presence of a catalyzer.

. 5. The process of hydrogenating composite fatty material and the likewhich comprises the sub-process of prior to hydrogenation diluting anoil containing material inhibiting catalyzer actiyity' with anotherSigned at Montclair in the county of Es- I oil substantially freefrom'inhibiting bodies. sex and State of New Jersey this 9th day 10 6.The process of hydrogeriiating cgmposof September A. D. 1912.v ite fattymaterial and the li e whic com- 5 prises diluting an oil containingcatalyzer I GARLETON ELLIS poison with another oil free from catalyzerWitnesses: poison and in atomizing the mixture with B. M. ELLIS,hydrogen in the presence of a catalyzer. L. MASON.

